CN112538198A - 一种抗菌流延pe-ld/pla可降解复合薄膜 - Google Patents
一种抗菌流延pe-ld/pla可降解复合薄膜 Download PDFInfo
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Abstract
本发明公开了一种抗菌流延PE‑LD/PLA可降解复合薄膜,由以下步骤制成:(1)PE‑LD和PLA塑料母粒需置于电热鼓风干燥机80℃中烘8小时;(2)将烘干的PE‑LD和PLA塑料颗粒按9:1—6:4质量比例混合,加入增容剂,再加入经过偶联剂改性的纳米TiO2,混合均匀后投入到双螺杆流延挤出机的喂料筒中;(3)当熔体从机头口模挤出时,先将其引入至冷却辊,并继续牵引至其他牵引装置后,经过拉伸,即可得到抗菌流延PE‑LD/PLA可降解复合薄膜。本发明将PE‑LD和PLA按比例混合,加入增容剂,并通过偶联剂将抗菌剂纳米TiO2加入到PE‑LD/PLA共混体系中,流延成膜。本发明所制备的可降解抗菌保鲜膜,具有很强的抗菌性能及良好的机械性能,可广泛用于食品保鲜、食品包装及其他生鲜包装等领域。
Description
技术领域
本发明涉及包装领域,具体涉及一种抗菌流延PE-LD/PLA可降解复合薄膜。
背景技术
食品保鲜膜在日常生活中应用广泛且对食品品质及安全意义重大。目前市面上常见的保鲜膜主要为不可降解的聚烯烃塑料薄膜,包括聚乙烯(PE)、聚丙烯(PP)聚氯乙烯(PVC),聚偏二氯乙烯(PVDC)等。这些聚烯烃类高分子都由石油裂解产物合成而来,属于不可再生资源,同时也是白色污染的主要成员。在呼声日益增长的低碳环保可持续发展战略下,逐步用可降解可持续的塑料制品替代不可降解的塑料,是社会发展的重要研究方向。
在众多可降解塑料中,PLA是最具前景的生物源塑料,利用可再生的植物资源(如玉米)所提出的淀粉原料制成,使用后能被自然界中微生物完全降解,最终生成二氧化碳和水,不污染环境,对保护环境非常有利,在医用材料领域有着非常重要的应用,在药物控制释放领域应用也比较普遍,已经显现出较大的商业价值。PE-LD是一种典型的柔而韧的聚合物,具有良好的熔融流动性,其物理、化学性能稳定且具有良好的生物相容性,因而在工农业生产等方面得到了广泛应用。PLA的熔融温度在150-180°C,与PE-LD的加工温度接近,两者的共混加工成为可能。一方面PLA可以为PE-LD提供强度,另一方面PE-LD可以对PLA进行增韧。在PE-LD中添加PLA使得整个体系成为可生物降解产品,可以在一定程度上减轻石油基塑料对环境的污染。但由于聚酯与聚烯烃的结构相差较大,所以二者的相容性是复合材料的一个较大问题,在共混过程中必须考虑使用增容剂。
在食品包装材料的应用中,活性包装目前越来越被市场认可,其中抗菌包装被广泛研究。纳米TiO2是一种优良的非溶出型抗菌剂,具有广谱抗菌性、长效性的特点,本身具有很好的化学稳定性和生物无毒性,在抗菌包装中的应用前景广阔。此外,TiO2具有较好的光催化能力,而且成本低廉,环境友好,因而被广泛用作光催化剂,在聚烯烃的降解中可以起良好的光催化作用,可与环境条件协同加速聚合物降解。
发明内容
本发明的目的在于克服现有技术的不足,提供一种具有很强抗菌性能及良好的机械性能的抗菌流延PE-LD/PLA可降解复合薄膜。
为了实现上述目的,本发明采用如下技术方案:
一种抗菌流延PE-LD/PLA可降解复合薄膜,由以下步骤制成:
(1)PE-LD和PLA塑料母粒需置于电热鼓风干燥机80℃中烘8小时;
(2)将烘干的PE-LD和PLA塑料颗粒按9:1—6:4质量比例混合,加入增容剂,再加入经过偶联剂改性的纳米TiO2,混合均匀后投入到双螺杆流延挤出机的喂料筒中;
(3)当熔体从机头口模挤出时,先将其引入至冷却辊,并继续牵引至其他牵引装置后,经过拉伸,即可得到抗菌流延PE-LD/PLA可降解复合薄膜。
作为优选的,在上述的抗菌流延PE-LD/PLA可降解复合薄膜中,步骤(1)中所述PE-LD为神华化工2426H或其他牌号的PE-LD,所述PLA为美国Natureworks4032D或其他牌号的PE-LD。
作为优选的,在上述的抗菌流延PE-LD/PLA可降解复合薄膜中,步骤(2)中所述增容剂为环氧大豆油、乙酰蓖麻油或分子量为1,000-8,000 Da的聚乙二醇中一种或者多种;增容剂的质量占混合塑料的总质量的2%-5%。
作为优选的,在上述的抗菌流延PE-LD/PLA可降解复合薄膜中,步骤(2)中所述的偶联剂为硅烷偶联剂。
作为优选的,在上述的抗菌流延PE-LD/PLA可降解复合薄膜中,步骤(2)中所述纳米TiO2的颗粒尺寸为5-10nm;纳米TiO2的添加量占混合塑料总质量的0.5%-5%。
与现有技术相比,本发明具有如下有益效果:本发明将PE-LD和PLA按比例混合,加入增容剂,并通过偶联剂将抗菌剂纳米TiO2加入到PE-LD/PLA共混体系中,流延成膜。本发明所制备的可降解抗菌保鲜膜,具有很强的抗菌性能及良好的机械性能,可广泛用于食品保鲜、食品包装及其他生鲜包装等领域。
附图说明
图1为实施例1-5的可降解流延PE-LD/PLA复合薄膜应力应变图。
图2为实施例1-5的可降解抗菌流延PE-LD/PLA复合薄膜的SEM图,其中PE-LD:PLA=80:20。
图3为实施例1的可降解抗菌流延PE-LD/PLA复合薄膜的DSC图。
具体实施方式
提供下列工作实施例纯粹是为了说明本发明的目的,不应被认为限制了所附权利要求所界定的保护范围。
实施例1:
将400.0g的PE-LD和100.0g的PLA塑料颗粒进行预混合,在其中加入20.0g的PEG-6000,量取5.0g的纳米TiO2于烧杯中并在其中滴0.1 mL硅烷偶联剂,搅拌均匀后加入到PE-LD和PLA混合体系中,再次搅拌均匀,倒入喂料筒中,开启双螺杆流延机的熔体泵、主机、喂料机,主机转速设置为10.0rpm,熔体泵转速设置为6.0rpm,料筒1-8区的温度设置为180℃-190℃,换网区、过渡体1-3区、熔体泵区温度设置为190℃-200℃,模头1-3区温度设置为210℃。流延拉伸辅机各个辊的线速度设置为1m/min。当熔体泵启动后开始牵膜,经流延辊、牵引辊、冷却辊、收卷辊得到复合膜产品。
本实施例制备的复合膜抗拉强度为15.12MPa,断裂伸长率为307.19%,屈服强度为8.16MPa。
实施例2:
将400.0g的PE-LD和100.0g的PLA塑料颗粒进行预混合,在其中加入20.0g的PEG-5000,量取10.0g的纳米TiO2于烧杯中并在其中滴入0.2 mL硅烷偶联剂,搅拌均匀后加入到PE-LD和PLA混合体系中,而后再次搅拌均匀,倒入喂料筒中,开启双螺杆流延机的熔体泵、主机、喂料机,主机转速设置为20.0rpm,熔体泵转速设置为10.0rpm,而其中的温度参数需提前设置,因为需要提前加热至设置温度,机器才能正常运行,料筒1-8区的温度设置为180℃-190℃,换网区、过渡体1-3区、熔体泵区温度设置为190℃-200℃,模头1-3区温度设置为210℃。流延拉伸辅机各个辊的线速度设置为2m/min。当熔体泵启动后开始牵膜,经流延辊、牵引辊、冷却辊、收卷辊得到复合膜产品。
本实施例制备的复合膜抗拉强度为12.61MPA,断裂伸长率为279.27%,屈服强度为7.10 MPa。
实施例3:
将400.0g的PE-LD和100.0g的PLA塑料颗粒进行预混合,在其中加入20.0g的PEG-4000,量取15.0g的纳米TiO2于烧杯中并在其中滴入0.3 mL滴硅烷偶联剂,搅拌均匀后加入到PE-LD和PLA混合体系中,再次搅拌均匀,倒入喂料筒中,开启双螺杆流延机的熔体泵、主机、喂料机,主机转速设置为20.0rpm,熔体泵转速设置为12.0rpm,料筒1-8区的温度设置为180℃-190℃,换网区、过渡体1-3区、熔体泵区温度设置为190℃-200℃,模头1-3区温度设置为210℃。流延拉伸辅机各个辊的线速度设置为2m/min。当熔体泵启动后开始牵膜,经流延辊、牵引辊、冷却辊、收卷辊得到复合膜产品。
本实施例制备的复合膜抗拉强度为9.51MPa,断裂伸长率为181.28%,屈服度为7.30MPa。
实施例4:
将400.0g的PE-LD和100.0g的PLA塑料颗粒进行预混合,在其中加入20.0g的PEG-6000,量取20.0g的纳米TiO2于烧杯中并在其中滴入0.3 mL硅烷偶联剂,搅拌均匀后加入到PE-LD和PLA混合体系中,再次搅拌均匀,倒入喂料筒中,开启双螺杆流延机的熔体泵、主机、喂料机,主机转速设置为20.0rpm,熔体泵转速设置为12.0rpm,料筒1-8区的温度设置为180℃-190℃,换网区、过渡体1-3区、熔体泵区温度设置为190℃-200℃,模头1-3区温度设置为210℃。流延拉伸辅机各个辊的线速度设置为2m/min。当熔体泵启动后开始牵膜,经流延辊、牵引辊、冷却辊、收卷辊得到复合膜产品。
本实施例制备的复合膜抗拉强度为12.65MPa,断裂伸长率为293.08%,屈服强度为8.54MPa。
实施例5:
将400.0g的PE-LD和100.0g的PLA塑料颗粒进行预混合,在其中加入20.0g的PEG-6000,量取25.0g的纳米TiO2于烧杯中并在其中滴入0.3 mL硅烷偶联剂,搅拌均匀后加入到PE-LD和PLA混合体系中,再次搅拌均匀,倒入喂料筒中,开启双螺杆流延机的熔体泵、主机、喂料机,主机转速设置为20.0rpm,熔体泵转速设置为12.0rpm,料筒1-8区的温度设置为180℃-190℃,换网区、过渡体1-3区、熔体泵区温度设置为190℃-200℃,模头1-3区温度设置为210℃。流延拉伸辅机各个辊的线速度设置为2m/min。当熔体泵启动后开始牵膜,经流延辊、牵引辊、冷却辊、收卷辊得到复合膜产品。
本实施例制备的复合膜抗拉强度为7.23MPa,断裂伸长率为121.49%,屈服强度为6.36MPa。
采用本发明所述制备方法制备的可降解抗菌保鲜膜进行膜抑菌实验按照以下步骤进行:
1、用接种针或接种环挑取菌种于液体培养基中,在37℃、150rpm下震荡培养20h。
2、将制备的可降解抗菌保鲜膜切成1.0cm直径的圆片,并在无菌条件下,用无菌水清洗5次,并将膜圆片平铺在制备好的5个培养皿上。
3、取步骤1培养的菌液用培养基稀释100倍,然后在每片步骤2制备的膜圆片上接入稀释后的菌液,涂匀,在37℃温度条件下培养过夜。用纯PE-LD膜作为对照。
进一步的,如表1所示,表1是采用本发明所述制备方法制备的可降解抗菌保鲜膜对不同细菌的抗菌活性。
表1 实施例1-5的可降解抗菌膜对不同细菌的抗菌活性
菌株 | PE | 1% TiO<sub>2</sub> | 2% TiO<sub>2</sub> | 3% TiO<sub>2</sub> | 4% TiO<sub>2</sub> | 5% TiO<sub>2</sub> |
大肠杆菌 | - | +++ | +++++ | +++++ | +++++ | +++++ |
金黄色葡萄球菌 | - | +++ | +++++ | +++++ | +++++ | +++++ |
注:TiO2以质量比添加PE-LD:PLA=80:20种;表中“-”代表无抗菌活性,“+’’代表强抗菌活性,“+’’越多代表抗菌活性越强5个“+’’为最大抗菌活性。
从表1可以看出PE-LD/PLA保鲜膜结合TiO2后,均对上述两种微生物具有显著的强抗菌活性,因此本发明制备的抗菌保鲜膜相比现有的保鲜膜对病原菌具有强抑杀作用。
Claims (5)
1.一种抗菌流延PE-LD/PLA可降解复合薄膜,其特征在于由以下步骤制成:
(1)PE-LD和PLA塑料母粒需置于电热鼓风干燥机80℃中烘8小时;
(2)将烘干的PE-LD和PLA塑料颗粒按9:1—6:4质量比例混合,加入增容剂,再加入经过偶联剂改性的纳米TiO2,混合均匀后投入到双螺杆流延挤出机的喂料筒中;
(3)当熔体从机头口模挤出时,先将其引入至冷却辊,并继续牵引至其他牵引装置后,经过拉伸,即可得到抗菌流延PE-LD/PLA可降解复合薄膜。
2.根据权利要求1所述的抗菌流延PE-LD/PLA可降解复合薄膜,其特征在于,步骤(1)中所述PE-LD为神华化工2426H或其他牌号的PE-LD,所述PLA为美国Natureworks4032D或其他牌号的PE-LD。
3.根据权利要求1所述的抗菌流延PE-LD/PLA可降解复合薄膜,其特征在于,步骤(2)中所述增容剂为环氧大豆油、乙酰蓖麻油或分子量为1,000-8,000 Da的聚乙二醇中一种或者多种;增容剂的质量占混合塑料的总质量的2%-5%。
4.根据权利要求1所述的抗菌流延PE-LD/PLA可降解复合薄膜,其特征在于,步骤(2)中所述的偶联剂为硅烷偶联剂。
5.根据权利要求1所述的抗菌流延PE-LD/PLA可降解复合薄膜,其特征在于,步骤(2)中所述纳米TiO2的颗粒尺寸为5-10nm;纳米TiO2的添加量占混合塑料总质量的0.5%-5%。
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